GOOD OPERATING PRACTICES

FOR

AMINE TREATING SYSTEMS

By

W. A. Smith
 This information is a tool for estimating some of the key operating

parameters of gas treating systems. The data is based on generally accepted

rules of thumb.

This manual contains four supplemental sections covering the operation of

Monoethanolamine (MEA), Diethanolamine (DEA), and Diglycolamine (DGA)

systems, and a section for establishing reflux rates for all amine stills and boiling

point curves for establishing reboiler temperatures.

The first three sections contain figures to provide quick determination of

amine circulation rates required as a function of gas volume and acid gas

content for each type of amine. Simple flow diagrams are also included for each

amine selection indicating typical operating parameters to be followed. An

example of a typical amine analysis report is provided indicating typical

operating ranges for rich acid gas pick up and lean residual solution acid gas

loadings.

The fourth section contains figures to establish amine reflux rates as a

function of gas volume and acid gas content and boiling point curves for the

typical amine solutions as a function of reboiler pressure to establish reboiler

temperatures.

All of this information is intended to help establish good operation

practices for amine treating systems. The following are general guidelines for

operation of amine treating processes. If assistance is needed for technical

guidance, contact your Plant/ Area Engineer.

Circulation Rates

Circulation of amine solution is determined by the acid gas content of the

inlet gas, strength of the solution, and the type of amine to be used. Figures 2,

3, 6, 7, 10, and 11 provide a quick determination of circulation required as a

function of gas volume and acid

gas content by type of amine. Solution strength used in these figures

represents those normally found in NGPLD operations; i.e., 15 percent MEA, 30

percent DEA, and 50 percent DGA. These concentrations should be maintained,

unless process design requirements are different, to ensure fuel requirements

for regeneration is minimized. Amine circulation can be calculated by the

following formulas:

For MEA; GPM = 41 x QXIZ

For DEA :GPM = 45 x

QXIZ

For DGA; GPM = 77 x

QXIZ

whereQ = Gas to be processed, MMSCFD

X = Acid gas content

= Mol% CO2 + Grains H2S/632

or

Mol% CO2 + Mol% H S

Z = Amine

concentration, wt. %

The above formulas were utilized to develop the Figures for amine

circulation rates and are based on mol loading of 0.33 mol acid gas/mol

amine for MEA, 0.5 mol acid gas/mol amine for DEA, and 0.3 mol acid

gas/mol amine for DGA. A good indicator of proper circulation rate is to

monitor the temperature of the rich amine leaving the

contactor. When amine reacts with H2S and CO2, heat is generated (exothermic

reaction) and, therefore, the rich amine temperature leaving the contactor

should be 20F. to 25F. hotter than the lean amine to the contactor.

Amine Still Operation

To reduce the H 2S content in the residue gas to pipeline specifications

requires the H2S in the lean amine to be stripped-to a very- low concentration.

"This can be accomplished by adding heat to the reboiler. The amount of heat

must be sufficient to increase the amine solution's temperature to its boiling

point. Since aqueous amine solutions boil at a constant temperature, Figures 14,

15, and 16 in Section Four can be used as a guide to establish reboiler

temperatures. Once this temperature has been established, excess heat must be

added. This heat will show as increased reflux.

The stripping of the amine for H 2S in the still is critical. Laboratory tests

of the lean amine should be made weekly to determine the amount of acid gas

left in the amine. This test is important. This laboratory test is called the lean

solution residual acid gas and reported as moles of acid gas per mole of amine

of lean solution. Figures 1, 5, and 9 show the acceptable ranges of lean solution

residual acid gas loading for various amine solutions.

The still can be producing low lean loading amine, but can also have a

corrosive condition that will eat out the trays in the still. Periodically,

simultaneous stripping tests should be run on the liquid from the still tower to

the reboiler and the lean amine from the reboiler. The residual concentrations

should be very near the same. If the residual is higher in the amine to the still

reboiler, it is an indication insufficient stripping is being

done in the still tower and part of the stripping is taking place in the reboiler. To

avoid this situation, the amount of heat to the reboiler must be increased to

generate sufficient steam to the still to perform principally all the acid gas

stripping in the still, with very little stripping of the acid gas from the amine being

done in the reboiler.

If the increased heat input does not help or correct the lack of stripping,

a check of the reflux rate should be made to determine if more heat is actually

being added to the reboiler. The reboiler heat controller may be indicating it has

increased the heat supply but, in actuality, it may have added very little or none.

The amount of reflux should increase if the heat input to the reboiler has

increased.

When the reflux does not have a meter, the volume can be determined by

lowering the liquid level in the reflux accumulator to near the bottom of the sight

glass, marking the level and shutting in the reflux pump. Check the time required

for the level to build up to a higher level. Calculate the gallons built up in the tank

and divide by the time in minutes to give gallons per minute reflux rate.

To help establish the required reflux rate Figure 13 in Section 4 can be

used when treater inlet gas volume and acid gas concentration is known. A good

"rule of thumb" for the amount of reflux required is 0.9 gallons per minute for

each 100,000 std. cubic feet per day acid gas produced when treating acid gas

with H 2S and CO 2 mixed. Acid gas that is high in CO2 and very little H 2S will

require about one-half the amount of reflux, that is 0.45 gallons per minute reflux

for each 100,000 std. cubic feet per day acid gas.

Controlling the heat to the reboiler can be accomplished by several

methods. The best method to control the heat to the reboiler is the still

overhead temperature. A temperature controller sensing the still top

temperature and controlling the heat into the

reboiler will give reasonable response to changes within the system. A change in

the heat to the reboiler and in still overhead composition will be detected and

controlled quickly.

When the stripping in the still is insufficient, all other checks show no

problems, increased heat to the reboiler, and increase reflux rate does not

improve stripping, then the problem is generally mechanical within the still tower.

To determine the problem will probably require an inspection of the tower

internals. Some of the problems can be:

(1) Dirty or partially plugged trays will reduce gas-liquid contact and

stripping efficiency. Badly plugged trays can cause high gas

velocities through the tray which can start flooding.

(2) Dirty or plugged packing if the still is packed.

(3) A loss of trays in the still will reduce stripping efficiency. The trays

may have been damaged by corrosion, blown loose or have come

loose and fallen down. This can happen anywhere within the tower,

from the top, through the middle or in the bottom.

(4) A loss of packing from the still will decrease stripping efficiency.

(5) Crushed packing can cause channeling through the still and reduce

stripping efficiency.

Amine Reclaimer

Heat stable salts, or thio-sulfates as noted on the laboratory amine

analysis sheets, Figures 1, 5, and 9, are formed when acidic compound

contaminants in the feed that are stronger than H 2S and CO 2, such as formic

acid, acetic acid, and sulfuric acid, react with

or degrade the amine to form heat-stable salts. The salts tie up the amine so

that it will no longer treat, and if their level builds enough, corrosion rates

increase in the system. The major gas contaminant is usually oxygen when it

reacts with amine and causes it to break down or degrade to organic acids,

which then form heat-stable salts. Periodic test should be run to ensure that

oxygen levels in the inlet gas streams are maintained at the lowest level possible.

During maintenance, be sure to purge all equipment with natural gas to remove

air before recharging equipment with amine solution. The amine surge tank

should have a natural gas blanket to prevent air from contacting the amine

solution.

Contaminated MEA solutions are purified by semi-continuous distillation in

a reclaimer. At the beginning of the reclaiming cycle, the reclaimer is filled with

lean amine solution. During the filling, a strong base, such as sodium carbonate

(Na 2CO3) or sodium hydroxide (NaOH), is added to the reclaimer to neutralize

the heat stable salts present in solution. The amount of soda ash to add is

generally 0.03 pounds per 12 gallons of initial fill. Heat is then added to the kettle

and water vapor and MEA are distilled off the top, leaving the contaminants in

the bottoms. A slipstream of one to three percent of the lean amine circulation

is continuously fed to the reclaimer until the liquid temperature in the reclaimer,

which rises as the contaminants accumulate, reaches 300F. The operation is

then stopped and the reclaimer is drained, terminating the cycle. The 300F.

temperature limit is set to minimize thermal degradation of the amine.

DEA has a higher boiling temperature than MEA. Consequently, in most

cases it is not practical, economical, or necessary to reclaim DEA solutions.

Solution purification
is maintained by mechanical and carbon filtration, and by caustic or soda ash

addition to the system to neutralize the heat stable amine salts.

DGA reclaimers utilize the same basic design techniques as those

employed for MEA reclaimers. To optimize reconversion of the DGA degradation

product, reclaiming is normally done at a temperature of 360-380F. A

supplemental water feed to the reclaimer is normally required in systems using

high--DGA concentrations-to limit the temperature in the reclaimer kettle to

380F. maximum. Control of the DGA feed to the reclaimer is usually

accomplished by setting a constant heat input to the reclaimer and then

controlling the reclaimer feed by means of a liquid level control.

Filters

A filtration scheme of mechanical and activated carbon filters is important

in maintaining good solution control. Mechanical filters such as cartridge filters

remove particulate material while carbon filters remove chemical contaminants

such as hydrocarbons, well treating compounds, pipeline corrosion inhibitors, iron

sulfide, etc.

A 10 to 20 micron mechanical filter should be adequate for particulate

removal. If cotton filters are used, the cotton should be virgin cotton rather

than recycled. Recycled cottons may contain fibers with coatings which may be

the source of amine solution foaming problems. The pressure drop across the

bed should be monitored, and when it reaches 5 psig to 10 psig, the filters

should be changed.

It is important to regenerate the charcoal filter frequently. The frequency

will depend upon the amount of contaminants in the gas and the size of the

filter, but should be at least often enough to keep the lean amine stream water

clear. When the amine

begins to turn an amber color or if foaming begins to appear, the charcoal beds

should be regenerated or replaced.

The charcoal filter should be regenerated by injecting steam into the top

of the bed and discharging the water and other effluents from the bottom. The

steam pressure should be held above 100 psig to give steam temperatures

above 300F. The higher the steam temperature held on the bed, the better the

bed will be generated. Steaming of the bed should continue until relatively clean,

clear water is drained from the bottom of the bed. The time required can be

from four hours to 24 hours.

Corrosion

When loaded with CO2 and H 2S, aqueous amine solutions can become

corrosive to carbon steel. Corrosion rates are increased by high amine

concentration, high acid gas loadings, high temperature degradation products,

and foaming. Also, corrosive are acid gases flashed from solution.

MEA is more reactive than DEA and DGA and, similarly, more corrosive.

The laboratory analysis, see Figures 1, 5, and 9, indicate acceptable ranges of

concentration for amine solutions and acid gas loadings. The corrosiveness of a

loaded amine solution is strongly influenced by the relative proportion of CO2 to

H 2S in the feed gas. CO2 is more corrosive to carbon steel than H 2S in aqueous

systems. Thus, for gases containing a higher ratio of CO 2 to H 2S, the rich acid

gas loading should be maintained at the lower end of the recommended loading

range. In a case where the feed gas is predominantly H2S, loadings at the higher

end of the loading range may be acceptable.

Foaming

Foaming is the most common problem of an amine plant operation. It can

be caused by solids floating in the liquid, well treating compounds, pipeline

corrosion inhibitors, heavy hydrocarbons, and other such contaminants that get

into the amine.

An immediate method to control a foaming problem in the still or

contactor is the addition of an antifoam at a location just upstream of the

vessel where the foaming problem exists. Effective foam inhibitors for amine

sweetening systems are silicone antifoams and polyalkylene glycols. Also, widely

used are high boiling alcohols such as oleylalcohol and octylphenomethanol. It is

advisable to test the antifoam on a plant sample in the laboratory before

applying it in the field to verify that it will break the foam.

The use of an antifoam is only a temporary solution to a continuing

problem. The objective should be to minimize the level of contaminants in the

amine solutions, reducing the cause of the problem. Therefore, the mechanical

and carbon filters should be checked to insure a clean solution is maintained. In

order to prevent hydrocarbons from condensing in the absorber/contactor, the

lean amine feed temperature should be held to 10F. above the temperature of

the feed gas. Amine solution strength should be checked. High amine strength

increases foaming tendency.

 REFERENCES

1. Butwell, K. F. and Kroop, L., "Fundamentals of Gas Sweetening", presented at

the 1983 Gas Conditioning Conference.

2. Campbell, Dr. J. M., Gas Conditioning and Processing, 1969

3. Dingman, J. C., "Gas Sweetening with Diglycolamine Agent", presented at the

Third Iranian Congress of Chemical Engineers organized by the School of
Engineering, Pahlavi University, Shiraz, Iran, November 6-10, 1977.

4. Dingman, J. C. and Moore, T. F., "Gas Sweetening with Diglycolamine",

presented at the Gas Conditioning Conference, University of Oklahoma,
Norman, Oklahoma, April 3, 1968

5. Gas Processors Suppliers Association, Engineering Data Book. Tenth Edition,

1987

6. Maddox, Dr. R N., Gas and Liquid Sweetening, 1974

7. Perry, C. R, Basic Design and Cost Data on MEA Treating Systems

8. Purgason, R S., "Fundamentals of Gas Treating", presented at the 1982

Gas Conditioning Conference